Oil detection process and apparatus

ABSTRACT

A process for detecting oil or lubricant contamination in a manufactured product, the process comprising adding a fluorescent taggant to oils or lubricants contained in processing machinery for said product, conveying said product past an infrared detection apparatus, irradiating said product with infrared radiation from said detection apparatus as it passes the detection apparatus, and detecting infrared radiation emitted from said irradiated product.

RELATED APPLICATION

This patent application is a continuation-in-part of U.S. Ser. No.13/338,971, filed on Dec. 28, 2011, (Attorney Docket 16083), and claimspriority to U.S. Provisional Application Ser. No. 61/490,403, filed onMay 26, 2011, (Attorney Docket 15785), the contents of each are herebyincorporated by reference in their entirety.

FIELD

Disclosed herein is an on-line inspection process and apparatus fordetection of oil and/or grease (lubricant) contamination on tobacco,tobacco products, food pharmaceuticals, packaging, and other consumergoods and products, and a light wavelength converting material fortaggant applications and quantitative diagnostics.

Environment

In the processing and packaging of consumer products and productsdesigned to provide tobacco enjoyment, oils, greases and lubricants mayinadvertently come into contact with the product being produced.

In the case of products designed to provide tobacco enjoyment, tobaccoleaf is processed prior to the time that it is provided as finalproduct. For example, leaf may be contacted by machinery duringharvesting, curing and transport to a stemmery. When leaf is provided instrip form at a stemmery, and cut or otherwise shredded to the desiredsize, it is possible for oils, greases and lubricants to inadvertentlycome into contact with the tobacco. Likewise, lubricants used inoperating the various machines used in the processing of the tobacco cancome inadvertently into contact with that tobacco. The sources oflubricant contamination can vary, such as when a particular piece ofmachinery or component of that piece of machinery fails to operate in anoptimum fashion.

Lubricants may inadvertently come into contact with tobacco due toleakage of lubricants through gaskets or seals, from sliding mechanisms,from drum systems, from gear boxes, from pumps, from sealed rollingbearing units, from chains and belts, and the like. Lubricants are usedin conditioning cylinders, threshers, separators, redryers, receivers,feeders, conveyors, cutters, blenders, tobacco presses and other suchpieces of equipment that are commonly used in tobacco stemmeries, and intobacco primary processing operations.

Lubricants of similar compositions are used throughout the variousstages of tobacco treatment and cigarette manufacture. Heretofore, ithas been difficult for the cigarette manufacturer to detect the presenceof oil in its tobacco and/or its cigarettes and to locate the source ofa particular lubricant once it has been detected.

It would be advantageous if the inspection of tobacco and tobaccoproducts for the presence of: a lubricant or the like could be conductedon-line, that is, in real time during the production process, with thecapability to identify the source, once it has been detected.

SUMMARY

In one aspect, disclosed is a process for detecting oil or lubricantcontamination in a manufactured product, the process comprising adding afluorescent taggant to oils or lubricants contained in processingmachinery for said product; conveying said product past an infrareddetection apparatus; irradiating said product with infrared radiationfrom said detection apparatus as it passes the detection apparatus; anddetecting infrared radiation emitted from said irradiated product.

In another aspect, disclosed is a process for detecting oil or lubricantcontamination in a tobacco product, the process comprising adding afluorescent taggant to oils or lubricants contained in tobaccoprocessing machinery; conveying tobacco product past an infrareddetection apparatus; irradiating said tobacco product with infraredradiation of a first wavelength from said detection apparatus as itpasses the detection apparatus; and detecting infrared radiation emittedfrom said irradiated tobacco product.

In yet another aspect, disclosed is a system for localization of oilcontamination, comprising a tipping machine for tobacco rods having aninfrared detection apparatus comprising a high intensity infrared lightsource directed at tobacco rods and a high speed NIR spectrometer sensortuned to detect an of a second wavelength emitted signal from anIndocyanine Green (ICG) complex disposed in said oil.

In a further aspect, disclosed is a process for detecting lubricantcontamination in a product produced by a manufacturing operation and/orprocessing operation. The process includes adding a first taggant to alubricant of a first machine of the operation, adding a second taggantto a lubricant of a second machine of the operation, and irradiating theproduct and detecting radiation emitted from the product responsivethereto, the detecting step including distinguishing the first taggantfrom the second taggant so as to discern the source of lubricantcontamination.

The irradiated product absorbs the original radiation and re-emitsradiation of a different wavelength than the original radiation, whichthen may be detected as disclosed herein.

BRIEF DESCRIPTION OF THE DRAWINGS

The forms disclosed herein are illustrated by way of example, and not byway of limitation, in the figures of the accompanying drawings and inwhich like reference numerals refer to similar elements and in which:

FIG. 1 is a block diagram showing the various stages in the process ofcigarette manufacturing;

FIG. 2 is a diagrammatic front elevational view of a filter tippingmachine which includes the detection apparatus of the present invention;

FIG. 3 is a detailed diagrammatic view of the detection apparatus of thepresent invention;

FIG. 4 is a representation of the infrared absorption and emission peaksof the Indocyanine Green (ICG) complex taggant, illustrating theStokes-shift;

FIG. 5 is a representation of the infrared absorption and emission peaksof a modified ICG-complex, illustrating a secondary emission peak;

FIG. 6 is a representation of the infrared absorption peak for themodified ICG-complex of Example 1; and

FIG. 7 is a representation of the infrared excitation and emission peaksfor the modified ICG-complex of Example 1; and

FIG. 8 is an H-nuclear magnetic resonance scan of the ICG-complexaccording to this invention.

DETAILED DESCRIPTION

Various aspects will now be described with reference to specific formsselected for purposes of illustration. It will be appreciated that thespirit and scope of the apparatus, system and methods disclosed hereinare not limited to the selected forms. Moreover, it is to be noted thatthe figures provided herein are not drawn to any particular proportionor scale, and that many variations can be made to the illustrated forms.Reference is now made to FIGS. 1-8, wherein like numerals are used todesignate like elements throughout.

Each of the following terms written in singular grammatical form: “a,”“an,” and “the,” as used herein, may also refer to, and encompass, aplurality of the stated entity or object, unless otherwise specificallydefined or stated herein, or, unless the context clearly dictatesotherwise. For example, the phrases “a device,” “an assembly,” “amechanism,” “a component,” and “an element,” as used herein, may alsorefer to, and encompass, a plurality of devices, a plurality ofassemblies, a plurality of mechanisms, a plurality of components, and aplurality of elements, respectively.

Each of the following terms: “includes,” “including,” “has,” “‘having,”“comprises,” and “comprising,” and, their linguistic or grammaticalvariants, derivatives, and/or conjugates, as used herein, means“including, but not limited to.”

Throughout the illustrative description, the examples, and the appendedclaims, a numerical value of a parameter, feature, object, or dimension,may be stated or described in terms of a numerical range format. It isto be fully understood that the stated numerical range format isprovided for illustrating implementation of the forms disclosed herein,and is not to be understood or construed as inflexibly limiting thescope of the forms disclosed herein.

Moreover, for stating or describing a numerical range, the phrase “in arange of between about a first numerical value and about a secondnumerical value,” is considered equivalent to, and means the same as,the phrase “in a range of from about a first numerical value to about asecond numerical value,” and, thus, the two equivalently meaning phrasesmay be used interchangeably.

It is to be understood that the various forms disclosed herein are notlimited in their application to the details of the order or sequence,and number, of steps or procedures, and sub-steps or sub-procedures, ofoperation or implementation of forms of the method or to the details oftype, composition, construction, arrangement, order and number of thesystem, system sub-units, devices, assemblies, sub-assemblies,mechanisms, structures, components, elements, and configurations, and,peripheral equipment, utilities, accessories, and materials of forms ofthe system, set forth in the following illustrative description,accompanying drawings, and examples, unless otherwise specificallystated herein. The apparatus, systems and methods disclosed herein canbe practiced or implemented according to various other alternative formsand in various other alternative ways.

It is also to be understood that all technical and scientific words,terms, and/or phrases, used herein throughout the present disclosurehave either the identical or similar meaning as commonly understood byone of ordinary skill in the art, unless otherwise specifically definedor stated herein. Phraseology, terminology, and, notation, employedherein throughout the present disclosure are for the purpose ofdescription and should not be regarded as limiting.

Disclosed hererin are new oil soluble, light wavelength-converting,preferably upconverting, compositions for taggant applications andquantitative diagnostics in connection with lubricants, such as by wayof non-limiting example, the detection of errant lubricants on productthat comes into contact with lubricated machinery. Other taggantapplications are contemplated, including, but not limited to,anti-counterfeiting, brand protection, or verification that a machinecontains a correct lubricant, and other possible applications. Adetection system enables the development of near real time, low cost,compact, portable and highly sensitive detection, monitoring anddiagnostics of modifications to manufacturing process systems in realworld environments. It is the unique process (e.g. the conversion ofvisible light to infrared light, infrared to visible light and theup-conversion of infrared to higher energy infrared) that enables highsensitivity detection against almost any sample or environmentalbackground.

Using the system, theoretical particle detection (10⁻²³ mol) ofmolecules added to analytic mixtures can be achieved through the use ofon-line verification methods and even handheld detection applications.Detection sensitivity of 10⁻²⁰ mol is possible in a variety of detectionschemes, and even direct visual detection of 10¹⁴ mol sensitivity hasbeen demonstrated using a hand held 3.0 to 9.0 volt laser diode systemagainst backgrounds of various colors and compositions. The narrowemission bandwidths and small particle size of these materials enablethe simultaneous detection of multiple analytes (i.e. multiplexedassays).

In one form, the detection system disclose herein can be used in manyprocesses and for consumer products which are susceptible to lubricantcontamination during the manufacturing process, such as for example inthe growing, collection, processing and/or packaging of packagedconsumer goods, such as food products, beverages, tipped and non-tippedcigars, cigarillos, snus and OTHER smokeless tobacco products, smokingarticles, electronic cigarettes, distilled products, pharmaceuticals,frozen foods and other comestibles, and the like. Further applicationscould include clothing, furniture, lumber or any other manufactured orpackaged product wherein an absence of oil is desired.

According to the present invention, a detectable taggant compound isadded to the various lubricants used in manufacturing and processingmachinery, and advantageously taggant compounds having differentcharacteristics are added into the lubricants at different processinglocations, such that detection of one or more of these taggant compoundscan enable rapid identification of the location of the source oflubricant contamination in the manufactured product.

Advantageously, the taggant compound is one which is detectable byfluorescence when it is exposed to particular wavelengths of light. Inparticular, a suitable taggant is one which absorbs energy at onewavelength and fluoresces/emits at a different wavelength. Suchmaterials are well-known in the art as Stokes-shifting materials, andhave recently found increasing use in inks for security marking ofdocuments, such as banknotes and the like, to render such documents lesssusceptible to counterfeiting or copying. However, some conventionalStokes-shifting and anti-Stokes conversion materials are composed ofinorganic compounds, such as doped rare earth metal particles, such asthose described in U.S. Published Patent Application No. 2010/0219377,which are insoluble in lubricants. It would be advantageous if taggantcompounds could be formulated to be soluble or dispersible in oils orlubricants.

In one form, the taggant may be an organic compound comprised ofpurified crystals from naturally occurring chlorophyll. Suitablenaturally-occurring chlorophyll crystals include Chlorophyll A (CASnumber 1406-65-1) and Chlorophyll B (CAS number 519-62-0). Thesetaggants are known as being down-converting or fluorescent, and aresensitive to a particular narrow wavelength of IR light (680nanometers). The taggant emits back this particular of light at adifferent wavelength (715 nanometers). A similar compound may be abenze-indolium perchlorate or a benze-indolium tosolyate. Such materialsabsorb around 670 nanometers and emit at a wavelength of 713 nanometers.Another material with down-conversion properties is Indocyanine Green(ICG). The chemical structure for Chlorophyll A is provided below.

Since this compound is an organic chemical, it is readily dissolved inoils and lubricants.

In another form, an oil-soluble fluorescent material has been developedbased on Indocyanine Green (ICG), the chemical structure of which isprovided below.

ICG is sodium4-[2-[(1E,3E,5E,7Z)-7-[1,1-dimethyl-3-(4-sulfonatobutyl)-benzo[e]indol-2-ylidene]hepta-1,3,5-trienyl]-1,1-dimethyl-benzo[e]indol-3-ium-3-yl]butane-1-sulfonate,an infrared fluorescing compound currently used in the medical industryfor imaging cells and blood flows in the human body, which in itsconventional form is water-soluble.

The newly developed taggant is an ICG-complex available from PersisScience LLC, Andreas Pa. The chemical structure for a tetrabutylammoniumchloride complexation of ICG is provided below and analytical structuralinformation is provided in FIG. 8.

The new ICG-complex is sensitive to a particular narrow absorption bandof IR light between about 760 to about 810 nanometers (FIG. 6), andemits light at a different band between about 810 to about 840nanometers (FIG. 7), with discrete absorbance peaks at about 785nanometers (FIG. 7) and 805 nanometers (FIG. 4), and a discrete emissionpeak at about 840 nanometers (FIG. 4).

The ICG complex can be added to oils or lubricants in the amounts ofapproximately 1 ppb to 5%, preferably a range of 1 ppm to 2000 ppm,based on the weight of the lubricant.

Additionally, the nature of the ICG complexing agent can be modified toimpart one or more secondary NIR emission wavelengths adjacent to themajor emission peak at 840 nanometers. By utilizing such variations inthe complexing agent, and adding differently complexed ICG compounds inlubricants at differing locations in the overall process, a singledetector can be located at the end of the process, and whencontamination is detected, the contaminated product can be removed fromthe process and further analyzed for the secondary NIR emission peaks,to determine the location of the source of contamination. FIG. 2 is anillustration of the absorption and emission peaks of a modifiedICG-complex, showing a secondary emission peak of a longer wavelength onthe shoulder of the primary emission peak.

In one form, the detection system of the present invention can be usedin many processes and for consumer products which are susceptible tolubricant contamination during the manufacturing process, such as forexample in the growing, collection, processing and/or packaging ofpackaged consumer goods, such as food products, beverages, tipped andnon-tipped cigars, cigarillos, snus and other smokeless tobaccoproducts, smoking articles, electronic cigarettes, distilled products,pharmaceuticals, cosmetics, foods and other consumer goods, and thelike. Further applications could include clothing, furniture, finishedwood or lumber or any other manufactured or packaged product wherein anabsence of oil spotting is desired.

In one form, the detection system utilizes near-infrared (NIR) emission,wherein a high intensity IR light source is directed at tobacco productsand emitted IR light from the taggant is gathered and analyzed using ahigh speed NIR spectrometer sensor tuned to detect the emission signalfrom the particular taggant added to the oil. Adequate measures are madeto prevent the detector from being able to see the excitationwavelength. This is done through the use of proper filters placed overthe detectors. The light from the laser is pulsed at a frequency ofabout 800 Hz and the detector is inversely pulsed to detect the taggant.NIR light can penetrate into various materials, such as tobacco rods, toa depth of several millimeters, even enabling subsurface inspection offinished cigarettes. The high speed NIR sensor can detect taggedoils/lubricants at speeds of over about 2,000 feet per minute or 4,000feet per minute or more. In the production of cigarettes, the high speedNIR sensor can detect tagged oils/lubricants of finished cigarettes at arate of 15,000 per minute (about 4,920 feet per minute), or even at arate of 20,000 per minute (about 6,560 feet per minute).

The high-speed detector comprises an IR laser diode that is used toexcite the taggant at its “absorption” frequency and a sensor that istuned to receive light at the taggant's “emission” frequency. If thesensor detects the presence of the taggant, it can change the state ofits output contacts. These output contacts can be used to stop themanufacturing equipment and set an alarm and/or to reject the oilcontaminated product.

The taggant can be added to process machinery lubricants atconcentrations between about 10 ppm and 100 ppm, typically at aconcentration of about 50 ppm, based on the weight of the oil/lubricant.At these taggant concentration levels the detection system can detect aslittle as 10 microliters of oil, or even as little as 1 microliter oftagged oil.

However, in order to provide for easier treatment of oils or lubricantsalready in place within various machines, it can be more convenient toformulate a master batch of the taggant in any particular oil, whereinthe taggant is mixed at higher concentrations in the base oil/lubricant,such as from about 0.1 to about 5 wt % taggant, or even from about 0.2to about 2 wt % taggant, in a balance of the base oil/lubricant. Aportion of such tagged master batch is then easily transported and addedto oils/lubricants which are already in place in the machines to betreated, for example by adding a small amount of the tagged master batchto the oil sump of the machine.

When the taggant is not an oil-soluble taggant, such as when it is aninorganic particle, an optional surfactant or dispersant additive can beadded in an amount effective to facilitate dispersion of the taggantparticles in the base oil. Such surfactants/dispersants are well-knownin the art and their identities need not be repeated herein.

The NIR emission detectors can be placed virtually anywhere along theprocess, such that a signal received by a detector at a known locationwill indicate oil contamination in the processed material almostimmediately, readily indicating the location of the source ofcontamination directly upstream of the detector.

In an alternative form, the nature of the ICG complexing agent can bemodified to impart one or more secondary NIR emission wavelengthsadjacent to the major wavelength peak at 840 nanometers. By utilizingsuch variations in the complexing agent, and adding differentlycomplexed ICG compounds in lubricants at differing locations in theoverall process, a single detector can be located at the end of theprocess, and when contamination is detected, the contaminated productcan be removed from the process and further analyzed for the secondaryNIR emission peaks, to determine the location of the source ofcontamination.

Referring now to FIG. 1, a block diagram showing the various stages inthe process of cigarette manufacturing is presented. As shown. Tobaccois first harvested at farm 10, which, in the case of tobacco for use incigarette manufacturing or the production of moist smokeless tobacco(MST), will be harvested at least in part by machinery. Tobacco in theform of leaf is baled and received at a receiving station 20 from farm10. Again, the opportunity exists for the tobacco bale to come intoinadvertent contact with lubricated machinery at receiving station 20.The baled tobacco may be transferred to a stemmery 30 wherein largestems are removed by machines to produce destemmed tobacco. Thedestemmed tobacco is packed into bales which are then stored for asuitable time period of up to several years. Destemmed tobacco is thentransferred to manufacturing center 40, wherein various types of tobaccostrip may be machine blended according to a predetermined recipe. Theblended tobacco may be treated by adding various flavorants to provide acased tobacco, which is then cut to provide tobacco “cut filler.”Various other types of tobacco can be added to the cut filler includingpuffed tobacco, reconstituted tobacco, tobacco reclaimed from rejectedcigarettes, and the like, to provide a final product blend. The blendmay be then fed to make/pack machine 50, which includes a continuouscigarette rod making apparatus. The continuous rod is then cut,optionally tipped, and packed, typically through the use of high-speedmachinery.

As may be appreciated from the above description, in tobacco processing,tobacco comes into contact with machinery at many different points inthe overall process, such as machinery used during the growing andharvesting operations on the farm, handling equipment at the receivingstation or auction house, machinery in the stemmery, on conveyors,conditioners, cutters and silos in the primary manufacturing centers,and ultimately on makers, tippers and packers in the make/packmanufacturing centers. By utilizing a different taggant in thelubricants of the machinery at each of these locations, the discretesource and/or location of contamination can be readily determined byinspection/detection of the finished product.

In FIG. 2, a typical filter tipping machine 100 for tobacco rods isshown, which comprises a frame supporting a rotary drum-shaped convey or101 having axially parallel peripheral flutes each of which contains asingle plain cigarette C of unit length. The cigarettes C in theneighboring flutes of the conveyor 101 are staggered with reference toeach other as seen in the axial direction of the conveyor 101, so thatthey form two rows each adjacent a different axial end of the conveyor101. Successive plain cigarettes C of one row are transferred intosuccessive flutes of one of two rotary drum-shaped aligning conveyors102, and the Cigarettes C of the other row are transferred intosuccessive flutes of the other aligning conveyor 102. The conveyors 102advance the respective plain cigarettes C at different speeds and/orthrough different distances to align each cigarette C of one row with acigarette C of the other row not later than at the transfer station atwhich successive axially aligned pairs of plain cigarettes C (with aclearance between their neighboring (inner) ends) are admitted intosuccessive axially parallel peripheral flutes of a rotary drum-shapedassembly conveyor 103.

A magazine or hopper 104 at the top of the frame of the filter tippingmachine contains a supply of filter rod sections of six times unitlength. The outlet of the magazine 104 admits discrete filter rodsections of six times unit length into successive axially parallelperipheral flutes of a rotary drum-shaped severing conveyor 106. Thelatter cooperates with two axially and circumferentially staggeredrotary circular knives 107 which subdivide each oncoming filter rodsection of six times unit length into groups of three coaxial filter rodsections of double unit length each.

Successive groups are delivered into the flutes of a composite rotarydrum-shaped staggering conveyor 108 which moves at least two filter rodsections of each group relative to each other and relative to the thirdfilter rod section in a circumferential direction and transferssuccessive filter rod sections of double unit length into successiveflutes of a rotary drum-shaped shuffling conveyor 109. The lattercooperates with suitable cams or the like (not shown) to form a singlerow of aligned filter rod sections which are advanced sideways intosuccessive flutes of a rotary drum-shaped combined accelerating andinserting conveyor 111. The conveyor 111 inserts discrete filter rodsections of double unit length into the aforementioned clearancesbetween successive pairs of plain cigarettes in the oncoming flutes ofthe assembly conveyor 103 so that each such flute of the conveyor 103which has advanced beyond the transfer station between the conveyors 103and 111 contains a group of three coaxial rod-shaped articles includingtwo axially spaced-apart tobacco rods of unit length and a filter rodsection of double unit length between them. Successive groups are causedto advance between two cams or the like (not shown) which cause thetobacco rods to move axially toward each other so that their inner endsabut the respective ends of the filter rod section between them. Thethus condensed or shortened groups are transferred into successiveflutes of a rotary drum-shaped transfer conveyor 112.

The frame of the filter tipping machine further supports an expiringreel 114 for a supply of an elongated web or strip 113 which isconvoluted onto the core of the reel 114. The web 113 is advancedlengthwise by rollers 116 which cause it to advance over the pronouncededge of a conventional curling tool 117, and a rotary drum-shapedsuction conveyor 119 thereupon causes the web 113 to advance into andbeyond a paster 118 serving to coat one side of the web with a film of asuitable adhesive. The adhesive-coated leader of the web 113 is severedat requisite intervals at the periphery of the suction conveyor 119 toyield a succession of adhesive coated discrete portions or uniting bandswhich are attached to successive groups of rod-shaped articles in theflutes of the transfer conveyor 112. Each uniting band extends along andslightly beyond both axial ends of the respective filter rod section ofdouble unit length.

Successive groups of rod-shaped articles (each such group carries auniting band) are transferred onto a drum-shaped rolling or wrappingconveyor 122 which cooperates with a normally stationary rolling member123 to convolute the uniting bands around the respective filter rodsections and around the adjacent inner ends of the respective pairs ofplain cigarettes C of unit length. The thus obtained filter cigarettes Cof double unit length are delivered into the flutes of a rotarydrum-shaped adhesive drying or setting conveyor 124 which, in turn,delivers successive filter cigarettes C of double unit length into theperipheral flutes of a rotary drum-shaped subdividing conveyor 126cooperating with a circular knife to sever each filter cigarette C ofdouble unit length midway across the tubular wrapper (converted orrolled uniting band) so that a conveyor 127 of a turn-around device 129receives pairs of coaxial filter cigarettes C of unit length. The device129 inverts one filter cigarette C of each pair end-for-end so that thesingle-length filter mouthpieces of all filter cigarettes C face in thesame direction not later than on a further conveyor 128 of theturn-round device 129 and the inverted and non-inverted filtercigarettes C form a single row of parallel cigarettes C which are causedto move sideways.

The conveyor 128 delivers successive filter cigarettes C of the singlerow into successive flutes of at least one inspection drum 131 which isfollowed by a combined testing and reject drum 132. As may beappreciated, the present invention contemplates the case in which eachflute of an inspection drum of a tipping machine receives twocigarettes. Any reference herein to a flute of an inspection drumreceiving a single cigarette is meant to cover such a case as well. Theinspection drum 131 can advance successive filter cigarettes C of unitlength past one or more NIR testing devices 140 each which irradiatescigarettes C with IR radiation having a wavelength of about 805 nm, anddetects reflected IR radiation at wavelengths at or about 840 nm (in thecase where the taggant is an ICG complex). As is conventional,inspection drum 131 may also be employed to detect loose ends, air leaksaround filter tips, etc. The reject drum 132 receives a signal from andcooperates with control device 140 to eject those filter cigarettes Cwhich are detected to contain one or more of the taggants according tothe present invention. A take-off conveyor (e.g., an endless belt orchain conveyor having an endless flexible element 136 trained overseveral pulleys, sheaves or sprocket wheels 134 of which only one isactually shown in FIG. 2) cooperates with a decelerating device 133 andserves to advance satisfactory filter cigarettes C of unit length to anext processing station, e.g., into a reservoir or into a packingmachine or to another destination.

FIG. 3 is a detailed illustration of inspection drum 131 which holds aseries of tipped cigarettes C on a fluted wheel via vacuum. Eachcigarette C is irradiated with IR radiation at a wavelength of about 805nm along the entire length of the cigarette C as it passes IR detectiondevice 140, and instantaneously emits IR radiation at wavelengths at orabout 840 nm from any tagged oil which might be contained in thecigarette C. The emitted IR radiation is in turn detected by IRdetection device 140, which sends a signal to reject drum 132 to rejectthe identified cigarette C.

FIG. 4 is an illustration of the absorption and emission peaks of thepresently disclosed ICG-complex taggant, and FIG. 5 an illustration ofthe absorption and emission peaks of a modified ICG-complex, showing asecondary emission peak of a longer wavelength on the shoulder of theprimary emission peak.

In one form, when the NIR detection device detects the presence of thetaggant primary emission peak, the identified cigarette is rejected andejected from the system. Subsequent to ejection, the cigarette can bere-analyzed with another NIR detection device which can identify thesecondary wavelength peaks from any of the variety ofdifferently-complexed ICG taggants, so as to determine the source oflubricant contamination throughout the system.

In another form, a process for detecting oil or lubricant contaminationin a manufactured product produced from raw materials is provided. Theprocess includes the steps of adding a first taggant to an oil orlubricant of a machine for preparing raw materials for a manufacturingoperation, adding a second taggant to an oil or lubricant of a machineused in a manufacturing operation for manufacturing the product,conveying the product past a detection apparatus adapted to distinguishthe first taggant from the second taggant so as to discern the source ofoil or lubricant contamination (i.e., whether the source of oil is fromproduction of a raw (or direct) material or from the production of thefinal product of which the raw material is a part). In one form, forexample and not by way of limitation, the first taggant is added, to theoil or lubricant of a machine for preparing raw materials for shipping.Further, for example and not by way of limitation, the second taggantmay be added to the oil or lubricant of a packaging machine. The productmay be irradiated with infrared radiation from the detection apparatusas it passes the detection apparatus and infrared radiation emitteddetected from the irradiated product. It is envisioned that if aplurality of machines are involved to produce a raw material, then aplurality of taggants would be utilized individually as to each of them.Likewise, if a plurality of machines is involved to produce the finalproduct, then a plurality of taggants would also be utilizedindividually as to each of them.

Specific forms will now be described further by way of example. Whilethe following examples demonstrate certain forms of the subject matterdisclosed herein, they are not to be interpreted as limiting the scopethereof, but rather as contributing to a complete description.)

EXAMPLES Example 1

500 mg of complexed ICG (Product No. OT-1013, available from PersisScience LLC of Andreas Pa.) is dispersed into 1.0 kg of Kluberoil 68using a speedmixer. Kluberoil 68 is available from Kluber LubricationNorth America L.P., Londonderry, N.H. The material is mixed for 10.0minutes at a speed of 2100 RPM. The resulting concentrate is slowlyadded to an additional 100.0 kg of Kluberoil 68 while stirring underhigh speed dispersion. A sample of the material is placed into aShimadzu 5301 Fluorometer and the excitation and emission spectrographsare recorded. When excited at a wavelength of 785, a strong infraredemission is noted from 810 nanometers to 960 nanometers. See FIG. 6 fora representation of the infrared absorption peak for the modifiedICG-complex of Example 1 and FIG. 7 for a representation of the infraredexcitation and emission peaks for the modified ICG-complex of Example 1.

Example 2

The above example is modified slightly using a tetrabutylammoniumbromide complexation of an Infrared dye available, IR830 available fromSigma-Aldrich of St. Louis, Mo. After mixing, it is noted that thematerial will produce fluorescence around 833 nanometers when excitedwith approximately 0.5 mW of 785 light.

Example 3

Upconverting nanoparticles, MED C-19 (Yb₂O₃:Er³⁺), were obtained fromPersis Science, LLC in a slurry format in DMSO. The DMSO was dialyzedfrom the aqueous phase leaving the particles in aqueous phase. Theparticles were dried and dispersed into Kluberoil 68 using a Speedmixer.The dispersion was measured optically using a Spex Fluorolog-3. The oilsuspension was excited at 970 nm and the detection occurred in thevisible from 400 to 700 nm to determine the presence of the tagged oil.

Example 4

0.5 wt % of a europium chelate, available from Honeywell Corporationunder the trade name of CD-335, was incorporated into 99.5 wt % ofLubriplate 220 oil using a horizontal media mill. Adequate detection wasachieved using UV LED's at a wavelength of 363 nm and an APD detectorwith a 600 nm-700 nm notch filter.

Example 5

1.0 wt % of an infrared abiorbing dithiolene dye commercially availablefrom Epolin, Inc—358 Adams St. Newark N.J. 07105, was dissolved viamixing with 99 parts of Kluber Oil 220 under nitrogen with a stir barfor 5 hours. The resulting mixture was analyzed for infrared absorption.The absorption occurred from 800 nm to 1200 nm with a peak at around1060 nm. The detection was achieved by contrast imaging with a CognexIn-Sight vision system and using a Monster LED light system with awavelength of 850 nm. A Midwest optical filter 850 bandpass was used toisolate the absorption.

As may be appreciated, other tobacco- and non-tobacco-related consumerproduct applications can benefit from the invention disclosed herein.Contemplated tobacco-related applications include cigars, cigarillos,MST, pouched tobacco products dry snuff, chewing tobacco and snus. Thetaggants disclosed herein may be applied in accordance with theseteachings to various machines and machine modules that execute variousmanufacturing operations at points along the manufacturing process ofinterest. The systems and methods disclosed herein can be modified forcompatibility with such applications.

While the present invention has been described and illustrated byreference to particular forms, those of ordinary skill in the art willappreciate that the invention lends itself to variations not necessarilyillustrated herein. For this reason, then, reference should be madesolely to the appended claims for purposes of determining the true scopeof the present invention.

1. A process for detecting oil or lubricant contamination in amanufactured product, the process comprising: adding a fluorescenttaggant to oils or lubricants contained in processing machinery for saidproduct; conveying said product past an infrared detection apparatus;irradiating said product with infrared radiation from said detectionapparatus as it passes the detection apparatus; and detecting infraredradiation emitted from said irradiated product.
 2. The process of claim1, wherein said taggant is a Stokes-shifting taggant, which absorbsinfrared radiation at a first wavelength and fluoresces at a secondwavelength, different from said first wavelength.
 3. The process ofclaim 2, wherein said first wavelength is about 805 nanometers and saidsecond wavelength is about 840 nanometers.
 4. The process of claim 1,wherein said product is a cigarette rod which is wrapped in paper. 5.The process of claim 1, wherein said product is a food product.
 6. Theprocess of claim 1, wherein the taggant is oil soluble.
 7. The processof claim 6, wherein the taggant is an Indocyanine Green complex.
 8. Theprocess of claim 1, wherein the taggant is added to said oils orlubricants at a concentration of between about 10 ppm and 100 ppm. 9.The process of claim 6, wherein the taggant is added to said oils orlubricants at a concentration of about 50 ppm.
 10. The process of claim1, wherein said detection step is conducted at a speed of about 2,000feet per minute or more.
 11. The process of claim 10, wherein saiddetection step is conducted at a speed of about 4,000 feet per minute ormore.
 12. A process for detecting oil or lubricant contamination in atobacco product, the process comprising: adding a fluorescent taggant tooils or lubricants contained in tobacco processing machinery; conveyingtobacco product past an infrared detection apparatus; irradiating saidtobacco product with infrared radiation from said detection apparatus asit passes the detection apparatus; and detecting infrared radiationemitted from said irradiated tobacco product.
 13. The process of claim12, wherein said taggant is a Stokes-shifting taggant, which absorbsinfrared radiation at a first wavelength and fluoresces at a secondwavelength, different from said first wavelength.
 14. The process ofclaim 13, wherein said first wavelength is about 805 nanometers and saidsecond wavelength is about 840 nanometers.
 15. The process of claim 12,wherein said tobacco product is a cigarette rod wrapped in paper. 16.The process of claim 12, wherein said tobacco product is a processedtobacco and said infrared detection device is located upstream of apackaging process.
 17. The process of claim 12, wherein the taggant isoil soluble.
 18. The process of claim 17, wherein the taggant is anIndocyanine Green complex.
 19. The process of claim 12, wherein thetaggant is added to said oils or lubricants at a concentration ofbetween about 10 ppm and 100 ppm.
 20. The process of claim 19, whereinthe taggant is added to said oils or lubricants at a concentration ofabout 50 ppm.
 21. The process of claim 12, wherein a detection level ofsaid tagged oils or lubricants is less than about 10 microliters. 22.The process of claim 21, wherein a detection level of said tagged oilsor lubricants is less than about 1 microliter.
 23. The process of claim12, wherein different fluorescent taggants are added to the oils orlubricants in different tobacco processing machinery.
 24. The process ofclaim 12, further comprising rejecting said tobacco product when saidmeasuring indicates the presence of said taggant.
 25. The process ofclaim 12, wherein said detection step is conducted at a speed of about2,000 feet per minute or more.
 26. The system of claim 25, wherein saiddetection step is conducted at a speed of about 4,000 feet per minute ormore.
 27. An inspection station for detecting oil or lubricantcontamination in a manufactured product, comprising (a) means foradvancing manufactured product; and (b) an infrared detection apparatus,said infrared detection apparatus including: (i) a high intensityinfrared light source for directing at the manufactured product and (ii)a high speed NIR spectrometer sensor tuned to detect an emitted signalfrom a taggant disposed in the oil, wherein said infrared detectionapparatus is positioned proximate said means for advancing manufacturedproduct at a distance effective to enable detection of reflected IRradiation as each advancing successive manufactured product isirradiated.
 28. The inspection station of claim 27, wherein the taggantis an Indocyanine Green complex.
 29. The inspection station of claim 27,wherein the Indocyanine Green complex disposed in the oil is aStokes-shifting taggant, which absorbs infrared radiation at a firstwavelength and fluoresces at a second wavelength, different from saidfirst wavelength.
 30. The inspection station of claim 29, wherein saidfirst wavelength is about 805 nanometers and said second wavelength isabout 840 nanometers.
 31. The inspection station of claim 29, whereinthe taggant is oil soluble.
 32. The inspection station of claim 31,wherein the taggant is added to the oil at a concentration of betweenabout 10 ppm and 100 ppm.
 33. The inspection station of claim 32,wherein the taggant is added to the oil at a concentration of about 50ppm.
 34. The inspection station of claim 32, wherein a detection levelof the tagged oil is less than about 10 microliters.
 35. The inspectionstation of claim 34, wherein a detection level of the tagged oil is lessthan about 1 microliter.
 36. The inspection station of claim 27, whereinthe infrared detection apparatus detects a primary emission peak of thetaggant.
 37. The inspection station of claim 36, wherein at least aportion of the manufactured product displaying the primary emission peakof the taggant are segregated for offline detection of a secondary peakassociated with a source of oil contamination.
 38. The inspectionstation of claim 27, wherein the infrared detection apparatus iseffective to detect subsurface oil contamination.
 39. The inspectionstation of claim 27, wherein the infrared detection apparatus iseffective to detect oil contamination at manufacturing speeds of 2,000feet per minute or more.
 40. The inspection station of claim 39, whereinthe infrared detection apparatus is effective to detect oilcontamination at manufacturing speeds of about 4,000 feet per minute ormore.
 41. The inspection station of claim 40, wherein the infrareddetection apparatus is effective to detect oil contamination atmanufacturing speeds of about 4,920 feet per minute.
 42. The inspectionstation of claim 41, wherein the infrared detection apparatus iseffective to detect oil contamination at manufacturing speeds of about6,560 feet per minute.
 43. The inspection station of claim 27, whereinsaid inspection station includes is an inspection drum of a cigarettetipping machine, said inspection drum having a plurality of flutes andsaid manufactured product is a tobacco rod.
 44. The inspection stationof claim 43, wherein each flute receives one or two tobacco rods forinspection.
 45. The inspection station of claim 44, wherein saidinspection drum advances successive tobacco rods past said high speedNIR spectrometer.
 46. The inspection station of claim 45, wherein saidtipping machine further comprises a reject drum, said reject drumconfigured to receive a signal from a control device to eject tobaccorods detected to contain one or more of the taggants.
 47. A process fordetecting oil or lubricant contamination in a product produced by amanufacturing operation and/or processing operation, comprising: addinga first taggant to an oil or lubricant of a first machine of theoperation; and irradiating the product and detecting radiation emittedfrom the product responsive thereto, wherein the first taggant issoluble or dispersible in the oil or lubricant and is a Stokes-shiftingtaggant, which absorbs radiation at a first wavelength and emitsradiation at a second wavelength, different from said first wavelength.48. The process of claim 47, wherein the operation includes preparing araw material for shipping.
 49. The process of claim 47, wherein theoperation includes a packaging machine.
 50. The process of claim 47,further comprising the steps of irradiating product with infraredradiation from a detection apparatus as it passes the detectionapparatus; and detecting infrared radiation emitted from the irradiatedproduct.
 51. A process for detecting oil or lubricant contamination inthe production of an article, comprising: adding an oil-soluble oroil-dispersible taggant to an oil or lubricant of a machine utilized toproduce the article or a component thereof.
 52. A process for detectingoil or lubricant contamination in the production of an article,comprising: adding an oil-soluble or oil-dispersible taggant-containingoil or lubricant to a machine utilized to produce the article or acomponent thereof.
 53. The process of claim 47, further comprising thestep of adding a second taggant to a lubricant of a second machine ofthe operation, wherein said detecting step further includesdistinguishing the first taggant from the second taggant so as todiscern the source of lubricant contamination.
 54. The process of claim51, wherein the taggant is a Stokes-shifting taggant, which absorbsinfrared radiation at a first wavelength and fluoresces at a secondwavelength, different from said first wavelength.
 55. The process ofclaim 54, wherein the taggant is an Indocyanine Green complex.
 56. Theprocess of claim 52, wherein the taggant of the taggant-containing oilor lubricant is a Stokes-shifting taggant, which absorbs infraredradiation at a first wavelength and fluoresces at a second wavelength,different from said first wavelength.
 57. The process of claim 55,wherein the taggant of the taggant-containing oil or lubricant is anIndocyanine Green complex.